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Results for “in situ electron microscopy”

Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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2,345 records
All sourcesNASA NTRSDOE OSTI
DOE OSTI2024

Real-space visualization of a defect-mediated charge density wave transition

Here, we study the coupled charge density wave (CDW) and insulator-to-metal transitions in the 2D quantum material 1T-TaS 2 . By applying in situ cryogenic 4D scanning transmission electron microscopy with in situ electrical resistance measurements, we directly visualize the CDW transition and establish that the transition is mediated by basal dislocations (stacking solitons). We find that dislocations can both nucleate and pin the transition and locally alter the transition temperature T c by nearly ~75 K. This finding was enabled by the application of unsupervised machine learning to cluster five-dimensional, terabyte scale datasets, which demonstrate a one-to-one correlation between resistance—a global property—and local CDW domain-dislocation dynamics, thereby linking the material microstructure to device properties. This work represents a major step toward defect-engineering of quantum materials, which will become increasingly important as we aim to utilize such materials in real devices.

4D-STEM↗
DOE OSTI2026

Machine learning pipeline for denoising low signal-to-noise ratio and out-of-distribution transmission electron microscopy datasets

High-resolution transmission electron microscopy (HRTEM) is crucial for observing material’s structural and morphological evolution at Angstrom scales, but the electron beam can alter these processes. Devices such as CMOS-based direct-electron detectors operating in electron-counting mode can be utilized to substantially reduce the electron dosage. However, the resulting images often lead to a low signal-to-noise ratio, which requires frame integration that sacrifices temporal resolution. Several machine learning (ML) models have been recently developed to successfully denoise HRTEM images. Yet, these models are often computationally expensive, and their inference speeds on GPUs are outpaced by the imaging speed of advanced detectors, precluding in situ analysis. Furthermore, the performance of these denoising models on datasets with imaging conditions that deviate from the training datasets has not been evaluated. To mitigate these gaps, we propose a new self-supervised ML denoising pipeline specifically designed for time-series HRTEM images. This pipeline integrates a blind-spot convolution neural network with pre-processing and post-processing steps, including drift correction and low-pass filtering. Results demonstrate that our model outperforms various other ML and non-ML denoising methods in noise reduction and contrast enhancement, leading to improved visual clarity of atomic features. Additionally, the model is drastically faster than U-Net-based ML models and demonstrates excellent out-of-distribution generalization. The model’s computational inference speed is in the order of milliseconds per image, rendering it suitable for application in in-situ HRTEM experiments.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Electron Microscopy Studies of Soft Nanomaterials

This review highlights recent efforts on applying electron microscopy (EM) to soft (including biological) nanomaterials. We will show how developments of both the hardware and software of EM have enabled new insights into the formation, assembly, and functioning (e.g., energy conversion and storage, phonon/photon modulation) of these materials by providing shape, size, phase, structural, and chemical information at the nanometer or higher spatial resolution. Specifically, we first discuss standard real-space two-dimensional imaging and analytical techniques which are offered conveniently by microscopes without special holders or advanced beam technology. The discussion is then extended to recent advancements, including visualizing three-dimensional morphology of soft nanomaterials using electron tomography and its variations, identifying local structure and strain by electron diffraction, and recording motions and transformation by in situ EM. On these advancements, we cover state-of-the-art technologies designed for overcoming the technical barriers for EM to characterize soft materials as well as representative application examples. Here, the even more recent integration of machine learning and its impacts on EM are also discussed in detail. With our perspectives of future opportunities offered at the end, we expect this review to inspire and stimulate more efforts in developing and utilizing EM-based characterization methods for soft nanomaterials at the atomic to nanometer length scales in academic research and industrial applications.

Imaging↗
DOE OSTI2025

Probing the role of local tunnel variations in early-stage lithiation of α-MnO₂ nanowires via in situ TEM

Understanding lithium-ion transport in tunnel-structured manganese oxides is essential for designing high-performance lithium-ion battery electrode materials. Here, we elucidate the early-stage lithiation mechanism of potassium-stabilized α-MnO 2 nanowires using in situ transmission electron microscopy (TEM) coupled with electron energy-loss spectroscopy (EELS), high-resolution TEM (HRTEM), and geometric phase analysis (GPA). Real-time TEM imaging reveals clear volume expansion at the reaction front, while EELS analysis uncovers lithium-ion diffusion far beyond this region, where no visible expansion is observed, indicating fast, defect-assisted transport. GPA and HRTEM analyses show that localized tensile and compressive strain fields, originating from pre-existing local tunnel structural variations, persist after lithiation. The tensile-strained regions enable lithium-ion insertion with minimal lattice distortion, offering additional free volume that facilitates rapid lithium-ion accommodation ahead of the structural transformation. Our results demonstrate a local tunnel variation-mediated fast diffusion pathway that precedes bulk reaction, underscoring the critical role of local strain in enabling early-stage lithium transport. Given the structural versatility of MnO 2 and its ability to accommodate diverse atomic arrangements beyond the well-known tunnel phases (β-, γ-, δ-, λ-, R-phases), our findings highlight the importance of understanding and engineering local structural environments. This work provides fundamental insights into the interplay between defects, strain, and ion dynamics, and presents defect engineering as a promising approach to enhance both rate performance and structural stability in manganese-based cathodes.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2024

Microscopy modality transfer of steel microstructures: Inferring scanning electron micrographs from optical microscopy using generative AI

Scanning electron microscopy (SEM) is resource intensive, which limits its throughput in some applications. As an alternative, we propose applying computer vision and machine learning to generate high-quality synthetic SEM micrographs from micrographs obtained using light optical microscopy (LOM). Working with a correlated LOM/SEM dataset of dual-phase steel images, we test generative models of various architectures, including encoder-decoder networks, generative adversarial networks (GANs), and diffusion-based models. We find that the diffusion models significantly outperform other methods on both qualitative and quantitative assessments, while preserving key metallurgical meaning. This work establishes diffusion as the state-of-the-art for microscopy modality transfer and demonstrates the potential of AI-powered microscopy to enhance LOM with micron scale structural recreation.

Computer vision↗
DOE OSTI2026

In situ studies on heavy ion irradiation and partial oxidation induced stacking faults and nanograins in tungsten nanolaminates

Understanding the microstructural evolution of tungsten (W) under extreme irradiation environments is critical for its application as a plasma-facing material in future fusion reactors. Heavy ion irradiation study offers expedited damage accumulation and thus allows irradiation tolerance property prediction in a short period of time. In this study we explore in situ Kr ion irradiation of W nanolaminates at 800 °C and uncover a complex interplay of irradiation-induced transformations, including the emergence of stacking faults, nanograin formation, and generation of thickened grain boundaries defined as GB regions with the thickness of up to 15 nm. High-resolution transmission electron microscopy studies reveal the formation of extended planar faults and a metastable hexagonal close-packed (hcp) phase within the body-centered cubic (bcc) matrix. These structural transitions are facilitated by irradiation-induced shear. They are further stabilized by the presence of oxygen, which promotes stacking fault formation and vacancy trapping. Elevated temperatures enhance defect mobility, enabling dynamic recrystallization into ultrafine grains and the thickening of GBs due to defect absorption and impurity segregation. These findings unravel non-equilibrium phase transformation pathways in heavy ion irradiated W and highlight the critical role of impurity-mediated defect dynamics in governing its radiation tolerance properties.

Wazeer, Adil [Purdue University]↗
DOE OSTI2026

NanoPSD: A software for automatic detection of Nano-Particle Shape Distribution in electron microscopy images

Accurate quantification of the size and morphology of nanoparticles from electron microscopy (EM) images is essential to understand growth mechanisms, surface reactivity, and functional behavior in nanoscale materials. Manual analysis remains slow, subjective, and difficult to reproduce in large datasets. We introduce NanoPSD (Nano-Particle Shape Distribution), an open-source and fully automated framework for quantitative particle detection and morphology analysis from EM images. NanoPSD integrates adaptive contrast enhancement, polarity-agnostic scale-bar detection, Optical Character Recognition (OCR)-based calibration, and classical segmentation via Otsu thresholding with morphological refinement. Particle contours are used to extract geometric descriptors, including equivalent circular diameter, aspect ratio, circularity, and solidity, enabling automated classification into spherical, rod-like, and aggregate morphologies. The framework supports both single-image and batch processing, generating publication-quality visualizations, LaTeX-ready tables, and structured comma-separated values (CSV) datasets. As a demonstration, we applied NanoPSD to plasma-synthesized nanoparticle samples diagnosed via transmission electron microscopy (TEM). The code produced statistically robust size and morphology distributions spanning a few to tens of nanometers with minimal user supervision. The pipeline demonstrates high reproducibility and scalability, processing large image collections with consistent calibration and output formatting. Its modular design enables seamless integration of future deep-learning-based segmentation models, providing a pathway toward intelligent, data-driven electron microscopy analysis.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Surface deposition of nanometer scale carbon structures on Bi 2 Sr 2 CaCu 2 O 8+δ using a low-cost scanning electron microscope

In this work, we investigate optically active nanostructures on Bi 2 Sr 2 CaCu 2 O 8+δ (BSCCO). The nanostructures are constructed from carbon nanocrystals formed using the electron beam of a scanning electron microscope to locally decompose residual hydrocarbons at the BSCCO surface. Atomic force microscopy is used to characterize the dimensions of these structures as a function of beam exposure time. This technique has been used to induce localized intercalation to form carbon nanoparticles up to tens of nanometers into a variety of 2D materials. Cross-sectional scanning transmission electron microscopy in BSCCO shows the presence of these carbon deposits on the surface, but there is no evidence they penetrate into the BSCCO substrate. Therefore, this technique is not suitable for localized intercalation in BSCCO, and it does have promise as a cost-effective approach to pattern nanometer scale etch stops.

2D materials↗
DOE OSTI2026

Ultrafast One-Dimensional Peierls-Distortion Dynamics in 1⁢T′−Re⁢S 2 Revealed by 4D Electron Microscopy

Rhenium disulfide (ReS 2 ), a prototypical 2D semiconductor with an anisotropic 1⁢T′ structure due to the pronounced Peierls distortion, has demonstrated great potential for polarization-dependent optoelectronics and photonics. Here, we report an ultrafast phase transition occurring within 1 ps, accompanied by a one-dimensional Peierls-distortion relaxation in 1⁢T′−ReS 2 revealed with combined 4D electron microscopy and time-dependent density functional theory calculations. Upon femtosecond laser pulse excitation, the Re-Re dimerization morphology rapidly transforms from a diamond cluster to zigzag chains and persists for several nanoseconds. Here, this ultrafast Peierls-distortion relaxation is further verified by transient changes in optical anisotropy via polarization-dependent transient absorption spectroscopy. Time-dependent density functional theory calculations attribute this novel phase transition to strong correlation between Peierls distortion and impulsive photoexcited carrier doping, predicting a transient band-gap collapse. This Letter opens up an exciting avenue for ultrafast control of Peierls-distortion-induced anisotropy and the metal-insulator transition in 1⁢T′−ReS 2 .

1T’-ReS2↗
DOE OSTI2026

The ABCs of phase retrieval: Connecting the acronyms of scanning transmission electron microscopy

High-resolution scanning transmission electron microscopy (S/TEM) is an indispensable tool for characterizing the structure and properties of materials down to the atomic scale. Conventional S/TEM imaging, however, is limited by the phase problem, whereby the phase of the electron exit wave is lost upon detection. Recent advances in diffractive imaging and 4D-STEM have enabled a range of phase-retrieval techniques that computationally reconstruct the missing information encoded in the phase of the transmission function. These approaches offer improved dose efficiency and enhanced sensitivity to weakly scattering signals, extending quantitative imaging to beam-sensitive materials composed of light elements. In this work, we introduce the phase problem in electron microscopy and survey the diverse landscape of phase-retrieval techniques used in the field. Despite their many acronyms and algorithmic variations, these techniques share a common physical and mathematical foundation. We present a unified framework that connects these seemingly distinct methods, from parallax imaging and tilt-corrected bright-field (tcBF-STEM), to aberration-corrected bright-field (acBF-STEM), optimum bright-field (OBF-STEM) and single-sideband (SSB) ptychography, as well as first-moment integrated center of mass techniques (iCOM) and iterative ptychographic algorithms. Based on these insights, we discuss the opportunities and practical limitations of applying these methods across different materials systems, detector designs, and microscope configurations.Graphical abstractRepresentative electron microscopy configurations used for phase retrieval and diffractive imaging in S/TEM: (a) Zernike phase-contrast transmission electron microscopy (TEM), (b) small-convergence-angle four-dimensional scanning transmission electron microscopy (4D-STEM) for nanobeam-based phase reconstruction methods, and (c) large-convergence-angle 4D-STEM for ptychographic and related diffractive imaging techniques reviewed in this work.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Realignment and suppression of charge density waves in the rare-earth tritellurides 𝑅⁢Te 3 (𝑅 = La, Gd, Er)

The rare-earth tritellurides have a rich phase diagram that includes charge density waves (CDWs), superconductivity, and magnetic order, offering a platform to study the interplay between these phases on a square-net system. Prior studies have shown that defects can affect the CDW characteristics in these materials, yet coupling between the CDW order and the underlying microstructure has not been studied at the nanoscale. Here we use scanning transmission electron microscopy at cryogenic temperatures to directly visualize the effects of defects on the CDW order and provide a spatially resolved microscopic correlation between the CDW transition and structural defects. Here, we show that in the presence of extended defects, such as dislocations and stacking faults, the weak orthorhombicity of the rare-earth tritellurides is lost and the material becomes pseudotetragonal. Since the orthorhombicity acts as a symmetry breaking field for the CDW transitions in rare-earth tritellurides, the presence of these extended defects modulates the energetics of the CDWs and suppresses the ground-state CDW phase at low temperature.

Charge density waves↗
DOE OSTI2024

4D-STEM Mapping of Nanocrystal Reaction Dynamics and Heterogeneity in a Graphene Liquid Cell

Chemical reaction kinetics at the nanoscale are intertwined with heterogeneity in structure and composition. However, mapping such heterogeneity in a liquid environment is extremely challenging. Here, in this work, we integrate graphene liquid cell (GLC) transmission electron microscopy and four-dimensional scanning transmission electron microscopy to image the etching dynamics of gold nanorods in the reaction media. Critical to our experiment is the small liquid thickness in a GLC that allows the collection of high-quality electron diffraction patterns at low dose conditions. Machine learning-based data-mining of the diffraction patterns maps the three-dimensional nanocrystal orientation, groups spatial domains of various species in the GLC, and identifies newly generated nanocrystallites during reaction, offering a comprehensive understanding on the reaction mechanism inside a nanoenvironment. This work opens opportunities in probing the interplay of structural properties such as phase and strain with solution-phase reaction dynamics, which is important for applications in catalysis, energy storage, and self-assembly.

four-dimensional scanning transmission electron mi↗
DOE OSTI2022

In Situ Tracking of Nonthermal Plasma Etching of ZIF-8 Films

Surface characterization is critical for understanding the processes used for preparing catalysts, sorbents, and membranes. Nonthermal plasma (NTP) is a process that achieves high reactivity at low temperatures and is used to tailor the surface properties of materials. In this work, we combine the capabilities of infrared reflection absorption spectroscopy (IRRAS) with NTP for the in situ interrogation of zeolitic imidazolate framework-8 (ZIF-8) thin films to probe modifications in the material induced by oxygen and nitrogen plasmas. The IRRAS measurements in oxygen plasma reveal etching of organic ligands with sequential removal of the methyl group and imidazole ring and with the formation of carbonyl moieties (C═O). In contrast, nitrogen plasma induces mild etching and grafting of nitrile groups (−C≡N). Scanning electron microscopy imaging shows that oxygen plasma, at prolonged times, significantly degrades the ZIF-8 film at the grain boundaries. Treatment of ZIF-8 membranes using mild plasma conditions yields a fivefold enhancement for H 2 /N 2 and CO 2 /CH 4 ideal selectivities and an eightfold enhancement for CO 2 /N 2 ideal selectivity. Additionally, the new tools described here can be used for spectroscopic in situ tracking of plasma-induced chemistry on thin films in general.

IRRAS↗
DOE OSTI2025

Methodology of Atomic Force Microscopy Visualization of Electrode–Electrolyte Interfaces

Electrochemical atomic force microscopy (EC-AFM) provides unprecedented insights into the microstructure of electrode–electrolyte interfaces during electrochemical reactions. However, performing EC-AFM measurements has many challenges, for example, drift, contamination, and probe degradation. We present solutions to these experimental issues through electrochemical cell design and carefully chosen experimental parameters. The possibility that the probes can react with the interface during scanning, generating false-positive electrochemical dynamics, is discussed as an example of the challenge of high-fidelity EC-AFM measurement. Here, we demonstrate this effect in highly ordered pyrolytic graphite and show that we could use electrochemical control of the AFM probe to enable high-fidelity in situ AFM visualization of solid–liquid interfaces during electrochemical reactions.

Electrochemical cells↗
DOE OSTI2026

Mapping the Microhardness of Al Matrix in U-7Mo/Al Dispersion Fuels at Medium and High Burn-up by in situ Nanoindentation

The mechanical degradation of the Al matrix in U-7Mo dispersion fuels was detected after irradiation in previous studies, but more details of the degradation mechanism are not clear yet to clarify the root cause. In this study, microhardness mapping in fresh and irradiated U-7Mo dispersion fuels coated with ZrN, with burn-up of 3.35 × 10 21 and 6.28 × 10 21 f/cm 3 , are measured to reveal the hardening of the Al matrix as a function of distance to fuel particles. Micro cubes were pulled by plasma focused ion beam scanning electron microscopy and tested by in situ nanoindenter with Berkovitch tip. Size effects are measured in medium and high burn-up samples. The higher burn-up specimen exhibits a more pronounced size effect when indent load is lower than 20 mN. Size effect correction models are also calculated by plots fitting, which predicts the true microhardness without size effect. Results shows that the hardness of the Al matrix near the ZrN coating has the highest value, then decreases moving away from the coating and become stable when the distance reaches ∼10 µm. The hardness starts increasing again getting closer to the next fuel particle, which makes the hardness distribution between two fuel particles to be “U” shape.

36 - MATERIALS SCIENCE↗
DOE OSTI2026

Visualizing Crystallization Dynamics and Transformation Pathways of Disordered Rocksalt Oxides During Thermally Activated Sol–Gel Synthesis

Sol–gel synthesis is a wet-chemical processing route for fabricating functional materials with control over composition and microstructure at relatively low temperatures compared to conventional solid-state synthesis. While sol–gel process initiates with intermixed molecular precursors, the early-stage nucleation pathways are insufficiently understood. Here, in this study, the chemical and structural transformation of ion disordered rocksalt (DRX) Li 1.2 Mn 0.4 Ti 0.4 O 2 (LMTO), a promising cathode material for lithium batteries, is studied by multiscale characterizations. In situ heating transmission electron microscopy (TEM) using a liquid cell visualizes and identifies crystallization pathways at the nanoscale. While some regions follow a classical multi-step transition through thermodynamically stable intermediates, others exhibit a kinetic shortcut via a localized amorphous matrix to directly form the DRX structure. Macroscale Fourier transform infrared spectroscopy corroborates the findings and reveals that transition metal ions are more strongly incorporated into the acetate-coordinated network than lithium. Although in situ heating TEM captures diverse local transformation pathways, in situ synchrotron X-ray diffraction indicates that the macroscopic transformation proceeds predominantly through spinel LMTO and lithium titanates toward DRX-LMTO. The findings uncover the spatiotemporal chemical and structural transformations in sol–gel derived DRX-LMTO materials, and call for fine-tuning of such sol–gel chemistries to manipulate the crystallization pathways and achieve target material homogeneity more efficiently.

cathode material↗
DOE OSTI2026

Atomic Evolution of Hydrogen Intercalation Wave Dynamics in Palladium Nanocrystals Revealed by Liquid-Phase Transmission Electron Microscopy

Solute-intercalation-induced phase separation creates spatial heterogeneities in host materials, a phenomenon ubiquitous in batteries, hydrogen storage, and other energy devices. Despite many efforts, probing intercalation processes at the atomic scale has been a significant challenge. By utilizing liquid-phase transmission electron microscopy (TEM), we study hydrogen (de)intercalation in palladium nanocrystals as a model system and have achieved unprecedented atomic-resolution imaging of hydrogen intercalation wave dynamics. Our observations reveal that intercalation wave mechanisms, instead of shrinking-core mechanisms, prevail at ambient temperature for palladium nanocubes ranging from ∼60 nm down to ∼10 nm. Systematic image analysis uncovers the atomic evolution of the hydrogen intercalation wave, transitioning from nonplanar and inclined boundaries to those closely aligned with {100} planes. Our kinetic Monte Carlo simulations demonstrate that the observed intercalation wave dynamics correspond to sorption pathways minimizing the lattice mismatch strain at the phase boundary. In conclusion, unveiling the atomic intercalation pathways holds profound implications for engineering intercalation-mediated devices and advancements in energy sciences.

Lee, Daewon [Lawrence Berkeley National Laboratory↗